Two types of coupled column-planar separation techniques will be developed as well as their applications in bioanalysis. Miniature- column high performance liquid chromatography (HPLC) will be combined with high performance thin layer chromatography (HPTLC) using a nebulizing interface. Bioanalytical applications of this configuration will be developed, such as lipid and polysaccharide class analyses, amino acid profiling of isoenzymes and bile acid analysis. A miniature elution device will be fabricated to permit laser-induced fluorescence detection of adsorbed solutes and also three dimensional separations. A second major type of coupled column-planar separation technique, HPLC X Electrophoresis, will be studied. After making both an evaluation of the compatibility of electrophoresis media with the nebulizing interface and any necessary modifications, several applications will be developed. These include HPLC X Isoelectric Focusing of protein digests and complex polynucleotide samples and Affinity Chromatography X Polyacrylamide Gel Electrofocusing of serum or cerebrospinal proteins. We anticipate that these methods will have marked influences in the areas of clinical, natural products and pharmaceutical chemistries, biotechnology and biochemistry.